CN115160007B - Carbon-carbon composite structure and preparation method thereof - Google Patents

Carbon-carbon composite structure and preparation method thereof Download PDF

Info

Publication number
CN115160007B
CN115160007B CN202210678626.2A CN202210678626A CN115160007B CN 115160007 B CN115160007 B CN 115160007B CN 202210678626 A CN202210678626 A CN 202210678626A CN 115160007 B CN115160007 B CN 115160007B
Authority
CN
China
Prior art keywords
carbon
composite structure
density
carbon composite
preset
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202210678626.2A
Other languages
Chinese (zh)
Other versions
CN115160007A (en
Inventor
刘时伟
胡士伟
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Zhejiang Dehong Carbon Fiber Composite Material Co ltd
Original Assignee
Zhejiang Dehong Carbon Fiber Composite Material Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Zhejiang Dehong Carbon Fiber Composite Material Co ltd filed Critical Zhejiang Dehong Carbon Fiber Composite Material Co ltd
Priority to CN202210678626.2A priority Critical patent/CN115160007B/en
Publication of CN115160007A publication Critical patent/CN115160007A/en
Application granted granted Critical
Publication of CN115160007B publication Critical patent/CN115160007B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71Ceramic products containing macroscopic reinforcing agents
    • C04B35/78Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80Fibres, filaments, whiskers, platelets, or the like
    • C04B35/83Carbon fibres in a carbon matrix
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/52Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
    • C04B35/522Graphite
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/52Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
    • C04B35/524Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from polymer precursors, e.g. glass-like carbon material
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/46Gases other than oxygen used as reactant, e.g. nitrogen used to make a nitride phase
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/608Green bodies or pre-forms with well-defined density
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74Physical characteristics
    • C04B2235/77Density

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Composite Materials (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Ceramic Products (AREA)

Abstract

The application relates to the technical field of carbon-carbon composite materials, in particular to a carbon-carbon composite structure and a preparation method thereof, wherein the method comprises the following steps: providing a tubular knitting mold, wherein a plurality of carbon fiber bundles are arranged on the side wall of the tubular knitting mold in the circumferential direction; weaving the carbon fiber based on a preset weaving path until the thickness of the carbon fiber layer reaches a first preset thickness; forming a carbon-carbon preform structure on a cylindrical braiding mold; carrying out high-temperature graphitization treatment on the carbon-carbon preform structure to obtain a low-density carbon-carbon composite structure with a three-dimensional interweaved frame; densifying, demolding and machining to obtain the target carbon-carbon composite structure; according to the method, the carbon fiber is woven through the weaving die, after high-temperature graphitization treatment, the low-density carbon-carbon composite structure with the three-dimensional interweaved frame is formed, the low-density carbon-carbon composite structure can be woven to the required thickness at one time, multi-layer adhesion is not needed, layering of the target carbon-carbon composite structure in the using process is avoided, and the service life of the target carbon-carbon composite structure is prolonged.

Description

Carbon-carbon composite structure and preparation method thereof
Technical Field
The application relates to the technical field of carbon-carbon composite materials, in particular to a carbon-carbon composite structure and a preparation method thereof.
Background
The carbon/carbon composite material is a carbon fiber reinforced carbon matrix composite material and has a series of excellent performances such as low density, high strength, high modulus, good fatigue resistance, good thermal shock performance and the like. In addition, the carbon/carbon composite material has excellent high-temperature mechanical property, the strength is not reduced and reversely increased along with the temperature rise, and researches show that the carbon/carbon composite material has strong fatigue resistance, and the strength is obviously better than that of a graphite product; the excellent performance of the carbon/carbon composite material mould makes the carbon/carbon composite material mould widely applied in the hot-pressing ceramic industry and gradually replaces graphite products.
At present, a 2.5D needling cylinder preform is adopted as a blank for preparing a carbon/carbon composite material hot-pressing ceramic die at home, densification is carried out by chemical vapor deposition, impregnation and other methods, the process has long manufacturing period, and the longitudinal cracking phenomenon of the die is caused by incomplete release of internal stress in the use process. The preform blank is also manufactured by a three-dimensional braiding molding process, and the method has high production cost and high consumption of manpower and material resources. And because of the limitation of the existing three-dimensional fabric technology, the size of the fabric is limited, the thickness is limited, the fabric needs to be adhered to a certain thickness by glue, but the adhesion force between the adhered fabric layers is weak, layering and cracking can occur after long-term use, and the service life of the product is seriously influenced.
Accordingly, there is a need to provide an improved carbon-carbon composite structure and a preparation scheme thereof to overcome the above-mentioned existing problems.
Disclosure of Invention
In order to solve the technical problem, the application provides a carbon-carbon composite structure and a preparation method thereof, and the application avoids layering of the carbon-carbon composite structure in the use process, ensures the strength of the carbon-carbon composite structure along the circumferential direction of the carbon-carbon composite structure, and prolongs the service life of the carbon-carbon composite structure.
The application discloses a preparation method of a carbon-carbon composite structure, which comprises the following steps:
s1: providing a tubular knitting mold, wherein a plurality of carbon fiber bundles are arranged on the side wall of the tubular knitting mold in the circumferential direction; wherein, gaps among the carbon fiber bundles form a preset knitting path with the knitting mould;
s2: braiding carbon fibers on the side wall of the braiding mold based on the preset braiding path until the thickness of the formed carbon fiber layer reaches a first preset thickness;
s3: spraying a resin curing agent on the carbon fiber layer, standing for a period of time, and forming a carbon-carbon preform structure on the cylindrical braiding mold;
s4: performing high-temperature graphitization treatment on the carbon-carbon preform structure to obtain a low-density carbon-carbon composite structure with a three-dimensional interweaved frame;
s5: and (3) densifying, demolding and machining the low-density carbon-carbon composite structure until the target carbon-carbon composite structure with the first preset density is obtained.
Further, the step S5 includes:
s51: carrying out vapor deposition on the low-density carbon-carbon composite structure by utilizing a resin carbon target material;
s52: carrying out impregnation and carbonization treatment on the carbon-carbon composite structure obtained after vapor deposition until the density of the low-density carbon-carbon composite structure reaches a second preset density, so as to obtain a high-density carbon-carbon composite structure;
s53: peeling the high-density carbon-carbon composite structure until the thickness of the high-density carbon-carbon composite structure is a second preset thickness;
s54: repeatedly executing step S52 on the high-density carbon-carbon composite structure subjected to peeling treatment until the density of the high-density carbon-carbon composite structure is in a preset density range;
s55: performing high-temperature graphitization treatment on the high-density carbon-carbon composite structure to obtain a carbon-carbon composite structure; wherein the preset density range includes the first preset density;
s56: and demolding and machining the carbon-carbon composite structure to obtain the target carbon-carbon composite structure with the first preset density.
Further, the said
Figure BDA0003695620060000021
The volume of the carbon-carbon preform structure=pi t (d+t), the ∈r->
Figure BDA0003695620060000022
Wherein D is the diameter of the tubular braiding mold, h is the height of the tubular braiding mold, D1 is the diameter of the carbon fibers, D2 is the diameter of the structure composed of a plurality of carbon fiber bundles, t is the thickness of the carbon-carbon preform structure, m is the weight of the carbon fibers, and k is the thickness of each unit layer in the carbon fiber layer.
Further, the first preset density and the preset range are each 1.5g/cm 3 -1.7g/cm 3 The second preset density is 1.2g/cm 3 -1.5g/cm 3
Further, the preset knitting paths include a first knitting path, a second knitting path, and a third knitting path; the step S2 includes:
the carbon fibers are subjected to cross knitting on the carbon fiber bundles according to the first knitting path, the second knitting path and the third knitting path on the side wall of the knitting mold until the thickness of the formed carbon fiber layer reaches a first preset thickness; the first knitting path is that the carbon fibers are knitted in a first direction, the second knitting path is that the carbon fibers are knitted in a second direction, the third knitting path is that the carbon fibers are knitted in a third direction, the third direction is the circumferential direction of the cylindrical knitting mold, and the first direction, the second direction and the third direction are mutually intersected.
Further, the distribution ratio of the carbon fibers woven in the first direction and the second direction to the carbon fibers woven in the third direction is (4-3): (6-7).
Further, the outer side of the carbon fiber bundles is also coated with a coating layer; the step S4 includes:
and carrying out high-temperature graphitization treatment on the carbon-carbon composite structure prefabricated body after standing, removing the coating layer through high-temperature graphitization treatment, and forming a supporting part along the length direction of the carbon fiber bundles by the carbon fiber bundles to obtain the low-density carbon-carbon composite structure with the three-dimensional interweaving frame.
Further, the diameter of the carbon fiber is 6.5-11mm, and the diameter of the carbon fiber bundle with the coating layer is 2-5mm.
Further, the outer diameter of the carbon fiber layer is 550-600mm, the first preset thickness is 100-150mm, and the height of the carbon fiber layer is 1000-1500mm; the volume density of the carbon fiber layer is 0.7-0.8g/cm 3
In another aspect, the present application also provides a carbon-carbon composite structure, which is prepared by the preparation method of the carbon-carbon composite structure.
Based on the technical scheme, the application has the following beneficial effects:
the method comprises the steps of braiding carbon fibers by using a braiding mold with carbon fiber bundles, and forming a low-density carbon-carbon composite structure with a three-dimensional interweaving frame after high-temperature graphitization treatment; the carbon-carbon composite structure with the three-dimensional interweaved frame can be woven to the required thickness at one time without multi-layer adhesion, so that layering of the carbon-carbon composite structure in the use process is avoided; meanwhile, the carbon-carbon composite structure with the three-dimensional interweaved frame improves the strength of the carbon-carbon composite structure along the circumferential direction, improves the phenomenon of column occurrence of the target carbon-carbon composite structure in the use process, and further improves the service life of the target carbon-carbon composite structure.
Drawings
In order to more clearly illustrate the technical solutions of the present application, the following description will make a brief introduction to the drawings used in the description of the embodiments or the prior art. It is obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained from these drawings without inventive effort for a person of ordinary skill in the art.
Fig. 1: the flow diagram of the preparation method of the carbon-carbon composite structure is provided;
fig. 2: the embodiment of the application provides a structure diagram of a carbon-carbon composite structure.
Detailed Description
The following description of the embodiments of the present application will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all, of the embodiments of the present application. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present application based on the embodiments herein.
For the following defined terms, these definitions shall be applied, unless a different definition is given in the claims or elsewhere in this specification. All numerical values, whether or not explicitly indicated, are defined herein as modified by the term "about". The term "about" generally refers to a range of values that one of ordinary skill in the art would consider equivalent to the stated value to produce substantially the same properties, functions, results, etc. A range of values indicated by a low value and a high value is defined to include all values included within the range of values and all subranges included within the range of values.
It should be noted that the terms "first," "second," and the like in the description and claims of the present application and the above figures are used for distinguishing between similar objects and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used may be interchanged where appropriate such that embodiments of the present application described herein may be implemented in sequences other than those illustrated or otherwise described herein. Furthermore, the terms "comprise" and "have," as well as any variations thereof, are intended to cover a non-exclusive inclusion.
The prior art has the following disadvantages: at present, a 2.5D needling cylinder preform is adopted as a blank for preparing a carbon/carbon composite material hot-pressing ceramic die at home, densification is carried out by chemical vapor deposition, impregnation and other methods, the process has long manufacturing period, and the longitudinal cracking phenomenon of the die is caused by incomplete release of internal stress in the use process. The preform blank is also manufactured by a three-dimensional braiding molding process, and the method has high production cost and high consumption of manpower and material resources. And because of the limitation of the existing three-dimensional fabric technology, the size of the fabric is limited, the thickness is limited, the fabric needs to be adhered to a certain thickness by glue, but the adhesion force between the adhered fabric layers is weak, layering and cracking can occur after long-term use, and the service life of the product is seriously influenced.
Aiming at the defects of the prior art, the application weaves carbon fibers by using a weaving die with carbon fiber bundles, and forms a low-density carbon-carbon composite structure with a three-dimensional interweaving frame after high-temperature graphitization treatment; the carbon-carbon composite structure with the three-dimensional interweaved frame can be woven to the required thickness at one time without multi-layer adhesion, so that layering of the carbon-carbon composite structure in the use process is avoided; meanwhile, the carbon-carbon composite structure with the three-dimensional interweaved frame improves the strength of the carbon-carbon composite structure along the circumferential direction, improves the phenomenon of column occurrence of the target carbon-carbon composite structure in the use process, and further improves the service life of the target carbon-carbon composite structure.
Referring to fig. 1, fig. 1 is a schematic flow chart of a preparation method of a carbon-carbon composite structure according to an embodiment of the present application. The present specification provides method operational steps as an example or a flowchart, but may include more or fewer operational steps based on conventional or non-inventive labor. The order of steps recited in the embodiments is merely one way of performing the order of steps and does not represent a unique order of execution. In the actual implementation of the preparation method, the method may be performed sequentially or in parallel according to the method shown in the embodiment or the drawings. The method comprises the following steps:
s1: providing a tubular knitting mold, wherein a plurality of carbon fiber bundles are arranged on the side wall of the tubular knitting mold in the circumferential direction; the gaps among the carbon fiber bundles form a preset weaving path with the weaving die;
s2: weaving carbon fibers on the side wall of the weaving die based on a preset weaving path until the thickness of the formed carbon fiber layer reaches a first preset thickness;
s3: spraying a resin curing agent on the carbon fiber layer, standing for a period of time, and forming a carbon-carbon preform structure on the cylindrical braiding mold;
s4: carrying out high-temperature graphitization treatment on the carbon-carbon preform structure to obtain a low-density carbon-carbon composite structure with a three-dimensional interweaved frame;
s5: and (3) densifying, demolding and machining the low-density carbon-carbon composite structure until the target carbon-carbon composite structure with the first preset density is obtained.
It should be noted that: in the present embodiment, a low-density carbon-carbon composite structure having a three-dimensional interlaced frame is formed by weaving carbon fibers using a weaving mold having carbon fiber bundles and performing high-temperature graphitization treatment; the carbon-carbon composite structure with the three-dimensional interweaved frame can be woven to the required thickness at one time without multi-layer adhesion, so that layering of the carbon-carbon composite structure in the use process is avoided; meanwhile, the carbon-carbon composite structure with the three-dimensional interweaved frame improves the strength of the carbon-carbon composite structure along the circumferential direction, improves the phenomenon of column occurrence of the target carbon-carbon composite structure in the use process, and further improves the service life of the target carbon-carbon composite structure.
In other possible embodiments, the resin curing agent includes a resin, an organic solvent, and a curing agent, the resin being a low viscosity resin or an epoxy resin.
Specifically, in the embodiment, a low-viscosity resin is used, the content ratio of the carbon fiber layer to the resin curing agent is 2:3, the curing time of an oven is 3-4 hours, and the curing temperature is 130-150 ℃; setting the carbon fiber layer at normal temperature for 6-8 hr; in the embodiment, the low-viscosity resin has good fluidity and is easy to permeate between carbon fiber layers, and meanwhile, the low-viscosity resin has low cost and high curing efficiency.
In some possible embodiments, step S5 includes:
s51: carrying out vapor deposition on the low-density carbon-carbon composite structure by utilizing a resin carbon target material;
s52: carrying out impregnation and carbonization treatment on the carbon-carbon composite structure obtained after vapor deposition until the density of the low-density carbon-carbon composite structure reaches a second preset density, so as to obtain a high-density carbon-carbon composite structure;
s53: peeling the high-density carbon-carbon composite structure until the thickness of the high-density carbon-carbon composite structure is a second preset thickness;
s54: repeatedly executing step S52 on the high-density carbon-carbon composite structure subjected to peeling treatment until the density of the high-density carbon-carbon composite structure is in a preset density range;
s55: performing high-temperature graphitization treatment on the high-density carbon-carbon composite structure to obtain a carbon-carbon composite structure; wherein the preset density range includes the first preset density;
s56: and demolding and machining the carbon-carbon composite structure to obtain the target carbon-carbon composite structure with the first preset density.
Specifically, performing impregnation and carbonization treatment on the carbon-carbon composite structure obtained after vapor deposition until the density of the low-density carbon-carbon composite structure reaches a second preset density, and obtaining the high-density carbon-carbon composite structure comprises:
heating the carbon-carbon composite structure obtained after vapor deposition to 800-1000 ℃ in an inert atmosphere environment, performing carbonization treatment, performing resin impregnation treatment on the carbonized carbon-carbon composite structure, and repeating carbonization and impregnation treatment processes until the density of the carbon-carbon composite structure reaches a second preset density to obtain the high-density carbon-carbon composite structure.
Further, vapor depositing the low density carbon-carbon composite structure with the resin carbon target includes:
placing the low-density carbon-carbon composite structure in the atmosphere of propylene and nitrogen, and performing vapor deposition treatment for 180-350h, wherein the deposition temperature is 800-1000 ℃, and the gas flow of the propylene and the nitrogen is 15-20l/min; the density of the low-density carbon-carbon composite structure can reach 1.2-1.35g/cm when vapor deposition is carried out for more than 300 hours 3 But the actual use density of the target carbon-carbon composite structure is 1.5-1.8g/cm 3 Therefore, the soaking-carbonization treatment is required to be repeated, so that the density is stably improved; generally, the density of the low-density carbon-carbon composite structure is increased by 0.1-0.2g/cm per one impregnation-carbonization process 3 The number of dip-carbonization processes is determined according to the product use density during the actual preparation process.
In other possible embodiments, the high temperature graphitization process in step S4 includes:
before power transmission and temperature rise, vacuumizing to more than 50Pa, closing a valve and a vacuum pump, keeping vacuum for 3h, and keeping the pressure rise rate less than 0.002MPa/3h;
when power is transmitted and the temperature is raised, the carbon-carbon preform structure is placed in a reaction device for high-temperature purification, the heating temperature is set to 2000-2400 ℃, a vacuum pump and a vacuum pumping valve are sequentially opened, and vacuum pumping is continuously carried out; after the temperature reaches 1800 ℃, charging protective gas for protection, continuously vacuumizing, always keeping the pressure in the furnace at about 3000pa, and uniformly heating for more than 30 hours;
performing heat preservation treatment on the carbon-carbon preform structure at 2000-2400 ℃, continuously filling protective gas for protection, continuously vacuumizing, always keeping the pressure in the furnace at about 3000pa, and continuously preserving heat for 5-6 hours;
after the heat preservation is finished, the reaction device is powered off and is cooled down freely, and after the temperature is lowered to below 800 ℃, forced cooling is performed; in the prior art, the heating and heat preservation temperature is (2000+/-20) DEG C, but when the carbon-carbon preform structure is put into a reaction device for high-temperature carbonization, the heat in the reaction device is easily emitted due to poor tightness between a box door and the reaction device, so that heat loss is caused; this may result in that the temperature cannot be maintained in an effective graphitization temperature range due to insufficient temperature of the reaction apparatus, and thus effective graphitization treatment cannot be achieved; the heating and heat preservation temperature of the embodiment is 2000-2400 ℃, so that the temperature of the reaction device is kept in an effective graphitization treatment temperature range, the graphitization effect is further achieved, and the mechanical property of the low-density carbon-carbon composite structure with the three-dimensional interweaved frame is improved.
In some possible embodiments, the first predetermined density and the predetermined range are each 1.5g/cm 3 -1.7g/cm 3 The second preset density is 1.2g/cm 3 -1.5g/cm 3
In other possible embodiments, step S52 includes:
placing the carbon-carbon composite structure subjected to vapor deposition treatment in an impregnating furnace, and vacuumizing to more than-0.09 MPa;
preheating impregnating resin to 60-65 ℃, sucking the preheated resin into an impregnating furnace, flushing protective gas, pressurizing to 1.4-1.6MPa, and impregnating for 2-3h;
decompression treatment is carried out on the impregnating furnace until the pressure in the impregnating furnace is 0.7-0.9MPa;
pressurizing the dipping furnace until the pressure in the dipping furnace is 1.4-1.6MPa;
controlling the temperature of the soaking furnace to rise to 60-120 ℃, and uniformly heating the soaking furnace within 3.5-4.5 hours;
the temperature of the dipping furnace is controlled to be continuously increased to 120-180 ℃ and is evenly increased within 4-6 hours;
controlling the temperature of the soaking furnace to be 180 ℃, and keeping the temperature for 1h;
placing the solidified carbon-carbon composite structure in a carbonization furnace, and controlling the temperature in the carbonization furnace to rise from room temperature to (200+/-10) DEG C, wherein the temperature is uniformly raised within 2.5-3.5 hours;
the temperature of the carbonization furnace is controlled to be continuously increased to (600+/-10) DEG C, and the temperature is uniformly increased within 35-45 h;
the temperature of the carbonization furnace is controlled to be continuously increased to (850+/-10) DEG C, and the temperature is uniformly increased within 10-15 hours;
the temperature of the carbonization furnace is controlled to be kept at (850+/-10) ℃, the heat preservation is continued for 1h, the carbon-carbon composite structure is controlled to be cooled along with the carbonization furnace, and the carbon-carbon composite structure is taken out of the carbonization furnace at the temperature of below 300 ℃ to finish carbonization treatment; wherein, the protection gas is continuously introduced for protection in the heating and cooling stages; the soaking and carbonization processes uniformly raise the temperature, and the air can be exhausted uniformly although the time is long, and the slow release of thermal stress is ensured, so that the target carbon-carbon composite structure with smaller deformation is obtained.
Specifically, the protective gas is nitrogen or argon, and the purity of the nitrogen or the argon is 99-99.999%.
Further, the carbon fibers are woven by using a weaving die with carbon fiber bundles, and after high-temperature graphitization treatment, a low-density carbon-carbon composite structure with a three-dimensional interweaving frame is formed, so that the carbon-carbon composite structure with the three-dimensional interweaving frame can be woven to a required thickness at one time without multi-layer bonding, and layering of the carbon-carbon composite structure in the use process is avoided; the proportion of the third-direction woven carbon fibers is increased, so that the strength of the third-direction woven carbon fibers in the circumferential direction is also improved, the phenomenon of longitudinal arrangement of the target carbon-carbon composite structure in the use process is improved, and the service life of the target carbon-carbon composite structure is prolonged; the density of the carbon-carbon composite structure with the three-dimensional interweaved frame is gradually increased to ensure the overall mechanical property of the carbon-carbon composite structure, so that the mechanical property of the carbon-carbon composite structure is prevented from being reduced compared with the mechanical property of the carbon-carbon composite structure with gradually increased density due to the fact that the density is greatly increased; meanwhile, when the density of the high-density carbon-carbon composite structure reaches a preset range, the hardness of the high-density carbon-carbon composite structure is reduced through high-temperature graphitization treatment, so that the cutter for the connection and disassembly processing is prevented from being damaged, the service life of the cutting cutter is prolonged, and the production cost is reduced.
Specifically, the demolding and machining process in step S56 includes:
separating the carbon-carbon composite structure from the cylindrical braiding mold, and performing demolding treatment; at this time, the carbon fiber bundles and the carbon fiber layer become a three-dimensional interweaved frame;
and (3) carrying out machining treatment on the demolded carbon-carbon composite structure, and cutting the demolded carbon-carbon composite structure into a plurality of target carbon-carbon composite structures.
It should be noted that: one carbon-carbon composite structure can be processed into a plurality of target carbon-carbon composite structures, and the carbon-carbon composite structures are different from the target carbon-carbon composite structures in size in that the height of the carbon-carbon composite structures is larger than that of the target carbon-carbon composite structures; one carbon-carbon composite structure can process a plurality of target carbon-carbon composite structures according to actual needs.
Specifically, the outer diameter of the target carbon-carbon composite structure is 500-550mm, the wall thickness of the target carbon-carbon composite structure is 100-120mm, and the height of the target carbon-carbon composite structure is 50-60mm.
In other possible embodiments, step S55 includes:
before power transmission and temperature rise, vacuumizing to more than 50Pa, closing a valve and a vacuum pump, keeping vacuum for 3h, and keeping the pressure rise rate less than 0.002MPa/3h;
when power is transmitted and the temperature is raised, the carbon-carbon preform structure is placed in a reaction device for high-temperature purification, the heating temperature is set to 2000-2200 ℃, a vacuum pump and a vacuum pumping valve are sequentially opened, and vacuum pumping is continuously carried out; after the temperature reaches 1800 ℃, charging protective gas for protection, continuously vacuumizing, always keeping the pressure in the furnace at about 3000pa, and uniformly heating for more than 30 hours;
performing heat preservation treatment on the carbon-carbon preform structure at 2000-2200 ℃, continuously filling protective gas for protection, continuously vacuumizing, always keeping the pressure in the furnace around 3000pa, and continuously preserving heat for 5-6 hours;
after the heat preservation is finished, the reaction device is powered off and is freely cooled, and after the temperature is reduced to below 800 ℃, the reaction device is forcedly cooled, and in the embodiment, the carbon-carbon composite structure obtained through densification treatment can reach 1.5g/cm 3 The carbon-carbon composite structure can reach 1.5g/cm 3 The cutter is damaged by the mechanical processing, so that the hardness of the carbon-carbon composite structure can be reduced by high-temperature graphitization, the mechanical processing can be performed, and the service life of the cutter can be prolonged.
In addition, the high-temperature graphitization treatment in the step S55 can also perform high-temperature purification on the carbon-carbon composite structure, has small influence on density, and can remove some metal and nonmetal impurities in the carbon-carbon composite structure obtained in the step S55 so as to enable the carbon-carbon composite structure to meet the purity requirement of customers.
Specifically, the reaction device comprises at least one of a vacuum smelting furnace, a vacuum sintering furnace, an ultra-high temperature graphitization furnace and a carbonization furnace.
In some possible embodiments, the preset knitting paths include a first knitting path, a second knitting path, and a third knitting path; the step S2 comprises the following steps:
on the side wall of the braiding mould, carbon fibers are subjected to cross braiding on carbon fiber bundles according to a first braiding path, a second braiding path and a third braiding path until the thickness of a formed carbon fiber layer reaches a first preset thickness; the first knitting path is formed by knitting carbon fibers in a first direction, the second knitting path is formed by knitting carbon fibers in a second direction, the third knitting path is formed by knitting carbon fibers in a third direction, the third direction is the circumferential direction of the tubular knitting mold, and the first direction, the second direction and the third direction are mutually intersected.
In some possible embodiments, the distribution ratio of carbon fibers woven in the first direction and the second direction to carbon fibers woven in the third direction is (4-3): (6-7), by increasing the proportion of the carbon fibers in the third direction, the circumferential strength of the target carbon-carbon composite structure is obviously improved, the situation that the target carbon-carbon composite structure is longitudinally cracked in the use process is avoided, and the service life of the target carbon-carbon composite structure is further prolonged.
In some of the possible embodiments of the present invention,
Figure BDA0003695620060000101
volume=pi t (d+t) of carbon-carbon preform structure, +.>
Figure BDA0003695620060000102
Wherein D is the diameter of the tubular braiding mold, h is the height of the tubular braiding mold, D1 is the diameter of the carbon fiber, D2 is the diameter of a structure composed of a plurality of carbon fiber bundles, t is the thickness of the carbon-carbon preform structure, and m is the weight of the carbon fiberThe amount, k, is the thickness of each unit layer in the carbon fiber layer.
Specifically, the density of the carbon-carbon preform structure is affected by the weight and volume of the carbon-carbon preform structure, and the density of the carbon-carbon preform structure is inversely proportional to the volume of the carbon-carbon preform structure and directly proportional to the weight of the carbon-carbon preform structure.
Further, the density of the carbon-carbon preform structure is proportional to the diameter of the cylindrical braiding mold, the height of the cylindrical braiding mold and the weight of the carbon fibers, and the density of the carbon-carbon preform structure is inversely proportional to the thickness of the carbon-carbon preform structure, the thickness of each unit layer in the carbon fiber layer, the diameter of the carbon fibers and the diameter of the structure composed of the plurality of carbon fiber bundles; namely, the larger the diameter of the cylindrical braiding mold, the height of the cylindrical braiding mold and the weight of the carbon fiber, the larger the density of the carbon-carbon preform structure; the smaller the thickness of the carbon-carbon preform structure, the thickness of each unit layer in the carbon fiber layer, the diameter of the carbon fiber, and the diameter of the plurality of carbon fiber bundles constituting the structure, the greater the density of the carbon-carbon preform structure.
It should be noted that: in the present embodiment, the density of the carbon-carbon preform structure can be changed by changing the diameter of the cylindrical braiding mold, the height of the cylindrical braiding mold, the weight of the carbon fibers, the thickness of the carbon-carbon preform structure, the thickness of each unit layer in the carbon fiber layer, the diameter of the carbon fibers, and the size of the diameters of the plurality of carbon-fiber bundle constituent structures; by improving the density of the carbon-carbon preform structure within a certain range, the mechanical property of the carbon-carbon preform structure can be improved, and meanwhile, the density of the carbon-carbon preform structure is improved within a proper range, so that the subsequent densification process is easier to densify to a required density range, and the production cost is reduced.
In some possible embodiments, the density of the carbon-carbon preform structure is 0.7-0.9g/cm 3 The diameter of the tubular braiding mold, the height of the tubular braiding mold, the weight of the carbon fibers, the density of the carbon-carbon preform structure and the thickness of the carbon-carbon preform structure, the thickness of each unit layer in the carbon fiber layer, the diameter of the carbon fibers and the diameter of the structure formed by a plurality of carbon fiber bundles are reasonably planned, so that the density of the carbon-carbon preform structure is 0.9 g%cm 3 The left and right sides enable the carbon-carbon preformed body structure to reach the maximum density, the mechanical property of the carbon-carbon preformed body structure can reach the optimal performance of the carbon-carbon preformed body structure, meanwhile, the carbon-carbon preformed body structure can be ensured to reach the first preset range by using fewer densification steps in the subsequent densification process, the densification steps are reduced to a certain extent, the production process is simplified, and the production cost is reduced.
Preferably, the formula for the density of the carbon-carbon preform structure applies to a first direction in which the angle between the carbon fibers and the side walls of the tubular braiding mold is 45 ° and a second direction in which the angle between the carbon fibers and the side walls of the tubular braiding mold is-45 °.
In some possible embodiments, the outside of the carbon fiber bundles is also coated with a coating layer; the step S4 includes:
performing high-temperature graphitization treatment on the carbon-carbon composite structure prefabricated body after standing, removing the coating layer through high-temperature graphitization treatment, and forming a supporting part along the length direction of the carbon fiber bundles by the carbon fiber bundles to obtain a low-density carbon-carbon composite structure with a three-dimensional interweaving frame; the strength of the cylindrical braiding mold is guaranteed through the arrangement of the coating layer, the cylindrical braiding mold is not easy to deform during braiding, and stability of the braiding process is guaranteed.
In some possible embodiments, the carbon fibers have a diameter of 6.5-11mm and the carbon fiber bundles with the cladding have a diameter of 2-5mm.
In some possible embodiments, the carbon fiber layer has an outer diameter of 550-600mm, a first predetermined thickness of 100-150mm, and a height of 1000-1500mm; the volume density of the carbon fiber layer is 0.7-0.8g/cm 3
Referring to fig. 2, fig. 2 is a structural diagram of a carbon-carbon composite structure.
In another aspect, the present application also provides a carbon-carbon composite structure, which is prepared by the method for preparing a carbon-carbon composite structure as described above.
The density of the carbon-carbon composite structure is more than or equal to 1.50g/cm 3 -1.70g/cm 3 Tensile strength of 170MPa-220MPa; the compressive strength is 147MPa to 170 MPa.
It should be noted that: the carbon-carbon composite structure prepared by the preparation method of the carbon-carbon composite structure has the advantages of high tensile strength, high compressive strength, light weight, high density, small thermal expansion coefficient and good thermal shock resistance, does not crack when being used in a rapid heating and quenching environment, and does not generate layering or longitudinal cracking during use, thereby prolonging the service life of the target carbon-carbon composite structure.
Example 1
S1: providing a tubular knitting mold, wherein a plurality of carbon fiber bundles are arranged on the side wall of the tubular knitting mold in the circumferential direction; the gaps among the carbon fiber bundles form a preset weaving path with the weaving die;
s2: weaving carbon fibers on the side wall of the weaving die based on a preset weaving path until the thickness of the formed carbon fiber layer reaches a first preset thickness;
s3: spraying a resin curing agent on the carbon fiber layer, placing the carbon fiber layer in an oven, keeping the temperature at 150 ℃, and standing for 4 hours to form a carbon-carbon preform structure on a cylindrical braiding mold;
s4: carrying out high-temperature graphitization treatment on the carbon-carbon preform structure to obtain a low-density carbon-carbon composite structure with a three-dimensional interweaved frame; wherein the high-temperature graphitization temperature is 2400 ℃;
s51: carrying out vapor deposition on the low-density carbon-carbon composite structure for 340h at 1000 ℃ by utilizing a resin carbon target material;
s52: repeating the dipping and carbonization treatment for 2 times on the carbon-carbon composite structure obtained after vapor deposition until the density of the low-density carbon-carbon composite structure reaches a second preset density, so as to obtain a high-density carbon-carbon composite structure; wherein the impregnation pressure is 1.4MPa, the impregnation is carried out for 2 hours, and the carbonization temperature is 850 ℃;
s53: peeling the high-density carbon-carbon composite structure until the thickness of the high-density carbon-carbon composite structure is a second preset thickness;
s54: repeatedly executing step S52 for 1 time on the high-density carbon-carbon composite structure after the peeling treatment until the density of the high-density carbon-carbon composite structure is in a preset density range;
s55: performing high-temperature graphitization treatment on the high-density carbon-carbon composite structure to obtain a carbon-carbon composite structure; wherein the preset density range includes the first preset density;
s56: and demolding and machining the carbon-carbon composite structure to obtain the target carbon-carbon composite structure with the first preset density.
In this example, the target carbon-carbon composite structure was 1.50g/cm 3 -1.6g/cm 3 At this time, the tensile strength of the target carbon-carbon composite structure is 170-200MPa or more, and the compressive strength is 147-154MPa or more.
Example 2
S1: providing a tubular knitting mold, wherein a plurality of carbon fiber bundles are arranged on the side wall of the tubular knitting mold in the circumferential direction; the gaps among the carbon fiber bundles form a preset weaving path with the weaving die;
s2: weaving carbon fibers on the side wall of the weaving die based on a preset weaving path until the thickness of the formed carbon fiber layer reaches a first preset thickness;
s3: spraying a resin curing agent on the carbon fiber layer, placing the carbon fiber layer in an oven, keeping the temperature at 150 ℃, and standing for 4 hours to form a carbon-carbon preform structure on a cylindrical braiding mold;
s4: carrying out high-temperature graphitization treatment on the carbon-carbon preform structure to obtain a low-density carbon-carbon composite structure with a three-dimensional interweaved frame; wherein the high-temperature graphitization temperature is 2400 ℃;
s51: carrying out vapor deposition on the low-density carbon-carbon composite structure for 340h at 1000 ℃ by utilizing a resin carbon target material;
s52: 2 times of dipping and carbonizing treatment are carried out on the carbon-carbon composite structure obtained after vapor deposition until the density of the low-density carbon-carbon composite structure reaches a second preset density, so that a high-density carbon-carbon composite structure is obtained; wherein, the dipping pressure is 1.6MPa, the dipping time is 3 hours, and the carbonization temperature is 860 ℃;
s53: peeling the high-density carbon-carbon composite structure until the thickness of the high-density carbon-carbon composite structure is a second preset thickness;
s54: repeatedly executing step S52 for 1 time on the high-density carbon-carbon composite structure after the peeling treatment until the density of the high-density carbon-carbon composite structure is in a preset density range;
s55: performing high-temperature graphitization treatment on the high-density carbon-carbon composite structure to obtain a carbon-carbon composite structure; wherein the preset density range includes the first preset density;
s56: and demolding and machining the carbon-carbon composite structure to obtain the target carbon-carbon composite structure with the first preset density.
In this example, the target carbon-carbon composite structure was 1.60g/cm 3 -1.63g/cm 3 At this time, the tensile strength of the target carbon-carbon composite structure is 200-205MPa or more, and the compressive strength is 154-165MPa or more.
Example 3
S1: providing a tubular knitting mold, wherein a plurality of carbon fiber bundles are arranged on the side wall of the tubular knitting mold in the circumferential direction; the gaps among the carbon fiber bundles form a preset weaving path with the weaving die;
s2: weaving carbon fibers on the side wall of the weaving die based on a preset weaving path until the thickness of the formed carbon fiber layer reaches a first preset thickness;
s3: spraying a resin curing agent on the carbon fiber layer, placing the carbon fiber layer in an oven, keeping the temperature at 130 ℃, and standing for 3 hours to form a carbon-carbon preform structure on a cylindrical braiding mold;
s4: carrying out high-temperature graphitization treatment on the carbon-carbon preform structure to obtain a low-density carbon-carbon composite structure with a three-dimensional interweaved frame; wherein the high-temperature graphitization temperature is 2000 ℃;
s51: carrying out vapor deposition on the low-density carbon-carbon composite structure for 180 hours at 800 ℃ by utilizing a resin carbon target material;
s52: repeating 2 times of dipping and carbonizing treatment on the carbon-carbon composite structure obtained after vapor deposition until the density of the low-density carbon-carbon composite structure reaches a second preset density to obtain a high-density carbon-carbon composite structureA combination structure; wherein the impregnation pressure is 1.4MPa, the impregnation is carried out for 2 hours, and the carbonization temperature is 850 ℃; at this time, the density of the high-density carbon-carbon composite structure was 1.38g/cm 3
S53: peeling the high-density carbon-carbon composite structure until the thickness of the high-density carbon-carbon composite structure is a second preset thickness;
s54: repeatedly executing step S52 for 2 times on the high-density carbon-carbon composite structure subjected to peeling treatment until the density of the high-density carbon-carbon composite structure is in a preset density range;
s55: performing high-temperature graphitization treatment on the high-density carbon-carbon composite structure to obtain a carbon-carbon composite structure; wherein the preset density range includes the first preset density;
s56: and demolding and machining the carbon-carbon composite structure to obtain the target carbon-carbon composite structure with the first preset density.
In this example, the target carbon-carbon composite structure was 1.58g/cm 3 -1.68g/cm 3 At this time, the tensile strength of the target carbon-carbon composite structure is 195-210MPa or more, and the compressive strength is 152-168MPa or more.
Example 4
S1: providing a tubular knitting mold, wherein a plurality of carbon fiber bundles are arranged on the side wall of the tubular knitting mold in the circumferential direction; the gaps among the carbon fiber bundles form a preset weaving path with the weaving die;
s2: weaving carbon fibers on the side wall of the weaving die based on a preset weaving path until the thickness of the formed carbon fiber layer reaches a first preset thickness;
s3: spraying a resin curing agent on the carbon fiber layer, placing the carbon fiber layer in an oven, keeping the temperature at 130 ℃, and standing for 3 hours to form a carbon-carbon preform structure on a cylindrical braiding mold;
s4: carrying out high-temperature graphitization treatment on the carbon-carbon preform structure to obtain a low-density carbon-carbon composite structure with a three-dimensional interweaved frame; wherein the high-temperature graphitization temperature is 2000 ℃;
s51: carrying out vapor deposition on the low-density carbon-carbon composite structure for 300h at 1000 ℃ by utilizing a resin carbon target material;
s52: repeating the dipping and carbonization treatment for 2 times on the carbon-carbon composite structure obtained after vapor deposition until the density of the low-density carbon-carbon composite structure reaches a second preset density, so as to obtain a high-density carbon-carbon composite structure; wherein the impregnation pressure is 1.4MPa, the impregnation is carried out for 2 hours, and the carbonization temperature is 850 ℃; at this time, the density of the high-density carbon-carbon composite structure was 1.38g/cm 3
S53: peeling the high-density carbon-carbon composite structure until the thickness of the high-density carbon-carbon composite structure is a second preset thickness;
s54: repeatedly executing step S52 for 3 times on the high-density carbon-carbon composite structure subjected to peeling treatment until the density of the high-density carbon-carbon composite structure is in a preset density range;
s55: performing high-temperature graphitization treatment on the high-density carbon-carbon composite structure to obtain a carbon-carbon composite structure; wherein the preset density range includes the first preset density;
s56: and demolding and machining the carbon-carbon composite structure to obtain the target carbon-carbon composite structure with the first preset density.
In the embodiment, the target carbon-carbon composite structure is 1.62-1.70g/cm 3 At this time, the tensile strength of the target carbon-carbon composite structure is 203-220MPa or more, and the compressive strength is 155-170MPa or more.
In summary, the application has the following beneficial effects:
(1) The method comprises the steps of braiding carbon fibers by using a braiding mold with carbon fiber bundles, and forming a low-density carbon-carbon composite structure with a three-dimensional interweaving frame after high-temperature graphitization treatment; the carbon-carbon composite structure with the three-dimensional interweaved frame can be woven to the required thickness at one time without multi-layer adhesion, so that layering of the carbon-carbon composite structure in the use process is avoided, the production cost is reduced, industrial production is facilitated, and the carbon-carbon composite structure has a higher market application scene.
(2) The carbon-carbon composite structure with the three-dimensional interweaved frame improves the strength of the carbon-carbon composite structure along the circumferential direction, improves the phenomenon of longitudinal columns of the target carbon-carbon composite structure in the use process, further improves the service life of the target carbon-carbon composite structure, reduces the production cost, is beneficial to industrial production, and has higher market application scenes.
The foregoing description has fully disclosed the embodiments of this application. It should be noted that any modifications to the specific embodiments of the present application may be made by those skilled in the art without departing from the scope of the claims of the present application. Accordingly, the scope of the claims of the present application is not limited to the foregoing detailed description.

Claims (8)

1. A method of making a carbon-carbon composite structure, the method comprising:
s1: providing a tubular knitting mold, wherein a plurality of carbon fiber bundles are arranged on the side wall of the tubular knitting mold in the circumferential direction; the gaps among the carbon fiber bundles form a preset weaving path with the weaving die, and the outer sides of the carbon fiber bundles are further coated with a coating layer;
s2: braiding carbon fibers on the side wall of the braiding mold based on the preset braiding path until the thickness of the formed carbon fiber layer reaches a first preset thickness; the preset knitting paths comprise a first knitting path, a second knitting path and a third knitting path; the step S2 includes: the carbon fibers are subjected to cross knitting on the carbon fiber bundles according to the first knitting path, the second knitting path and the third knitting path on the side wall of the knitting mold until the thickness of the formed carbon fiber layer reaches a first preset thickness; the first knitting path is that the carbon fibers are knitted in a first direction, the second knitting path is that the carbon fibers are knitted in a second direction, the third knitting path is that the carbon fibers are knitted in the circumferential direction of the knitting mold, the circumferential direction of the knitting mold is a third direction, and the first direction, the second direction and the third direction are mutually intersected;
s3: spraying a resin curing agent on the carbon fiber layer, standing for a period of time,forming a carbon-carbon preform structure on the cylindrical braiding mold; wherein the density of the carbon-carbon preform structure is 0.7-0.9g/cm 3
S4: performing high-temperature graphitization treatment on the carbon-carbon preform structure to obtain a low-density carbon-carbon composite structure with a three-dimensional interweaved frame;
s5: densifying, demolding and machining the low-density carbon-carbon composite structure until a target carbon-carbon composite structure with a first preset density is obtained; the step S5 includes:
s51: carrying out vapor deposition on the low-density carbon-carbon composite structure by utilizing a resin carbon target material;
s52: carrying out impregnation and carbonization treatment on the carbon-carbon composite structure obtained after vapor deposition until the density of the low-density carbon-carbon composite structure reaches a second preset density, so as to obtain a high-density carbon-carbon composite structure;
s53: peeling the high-density carbon-carbon composite structure until the thickness of the high-density carbon-carbon composite structure is a second preset thickness;
s54: repeatedly executing step S52 on the high-density carbon-carbon composite structure subjected to peeling treatment until the density of the high-density carbon-carbon composite structure is in a preset density range;
s55: performing high-temperature graphitization treatment on the high-density carbon-carbon composite structure to obtain a carbon-carbon composite structure; wherein the preset density range includes the first preset density;
s56: and demolding and machining the carbon-carbon composite structure to obtain the target carbon-carbon composite structure with the first preset density.
2. The method for producing a carbon-carbon composite structure according to claim 1, wherein the weight of the carbon-carbon preform structure is =
Figure QLYQS_1
Volume=pi t (d+t) of the carbon-carbon preform structure, density of the carbon-carbon preform structure = = -j =>
Figure QLYQS_2
The method comprises the steps of carrying out a first treatment on the surface of the Wherein D is the diameter of the tubular braiding mold, h is the height of the tubular braiding mold, D1 is the diameter of the carbon fibers, D2 is the diameter of the structure composed of a plurality of carbon fiber bundles, t is the thickness of the carbon-carbon preform structure, m is the weight of the carbon fibers, and k is the thickness of each unit layer in the carbon fiber layer.
3. The method of claim 1, wherein the first predetermined density and the predetermined density range are each 1.5g/cm 3 -1.7g/cm 3 The second preset density is 1.2g/cm 3 -1.5g/cm 3
4. The method of producing a carbon-carbon composite structure according to claim 1, wherein a distribution ratio of the carbon fibers woven in the first direction and the second direction to the carbon fibers woven in the third direction is (4-3): (6-7).
5. The method for producing a carbon-carbon composite structure according to claim 1, wherein the step S4 includes:
and carrying out high-temperature graphitization treatment on the carbon-carbon composite structure prefabricated body after standing, removing the coating layer through high-temperature graphitization treatment, and forming a supporting part along the length direction of the carbon fiber bundles by the carbon fiber bundles to obtain the low-density carbon-carbon composite structure with the three-dimensional interweaving frame.
6. The method for producing a carbon-carbon composite structure according to claim 5, wherein the diameter of the carbon fiber is 6.5 to 11mm, and the diameter of the carbon fiber bundle having the coating layer is 2 to 5mm.
7. The method for preparing a carbon-carbon composite structure according to claim 1, wherein the outer diameter of the carbon fiber layer is 550-600mm, the first preset thickness is 100-150mm, and the height of the carbon fiber layer is 1000-1500mm; bulk density of the carbon fiber layer0.7-0.8g/cm 3
8. A carbon-carbon composite structure, characterized by being produced by the method for producing a carbon-carbon composite structure according to any one of claims 1 to 7.
CN202210678626.2A 2022-06-15 2022-06-15 Carbon-carbon composite structure and preparation method thereof Active CN115160007B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210678626.2A CN115160007B (en) 2022-06-15 2022-06-15 Carbon-carbon composite structure and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210678626.2A CN115160007B (en) 2022-06-15 2022-06-15 Carbon-carbon composite structure and preparation method thereof

Publications (2)

Publication Number Publication Date
CN115160007A CN115160007A (en) 2022-10-11
CN115160007B true CN115160007B (en) 2023-06-06

Family

ID=83485737

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210678626.2A Active CN115160007B (en) 2022-06-15 2022-06-15 Carbon-carbon composite structure and preparation method thereof

Country Status (1)

Country Link
CN (1) CN115160007B (en)

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5127783A (en) * 1989-05-25 1992-07-07 The B.F. Goodrich Company Carbon/carbon composite fasteners
CN1482098A (en) * 2003-07-24 2004-03-17 上海交通大学 Process for preparing carbon-to-carbon composite material
CN1255571C (en) * 2004-05-13 2006-05-10 上海交通大学 Carbon-carbon/aluminium composite material preparation method
KR20120094136A (en) * 2009-12-17 2012-08-23 도레이 카부시키가이샤 Layered carbon-fiber product, preform, and processes for producing these
CN104311093A (en) * 2014-09-26 2015-01-28 内蒙古航天红岗机械有限公司 Preparation method of C/C composite material
CN107382355A (en) * 2017-07-24 2017-11-24 苏州宏久航空防热材料科技有限公司 A kind of fine and close C/C composite material and preparation method thereofs
CN110105077A (en) * 2019-04-10 2019-08-09 嘉兴启晟碳材料有限公司 A kind of technique using rim charge production carbon carbon composite board
CN114560715B (en) * 2022-04-28 2022-10-14 浙江德鸿碳纤维复合材料有限公司 Crucible supporting rod and preparation method thereof

Also Published As

Publication number Publication date
CN115160007A (en) 2022-10-11

Similar Documents

Publication Publication Date Title
CN111170756B (en) Preparation method of revolving body carbon/carbon composite material
CN110372390B (en) Preparation method of continuous fiber reinforced SiC part based on additive manufacturing and product
CN101948327A (en) Method for preparing work hardening insulation quilt for high temperature furnace
CN108101566B (en) Method for preparing silicon carbide ceramic matrix composite component with assistance of RTM (resin transfer molding) process
CN113024269A (en) Preparation method of high-performance super-large and super-thick carbon/carbon composite material
CN111848203A (en) Method and die for net size forming of carbon fiber needling preform
CN111875401B (en) Preparation method of high-strength and high-purity carbon/carbon composite material revolving body formed by winding
CN114379115A (en) Carbon crucible support and preparation method thereof
CN115448744B (en) Preparation method of carbon/carbon throat liner
CN112479731A (en) Preparation method of carbon fiber sewing hardening heat-insulation material
CN113061046A (en) Preparation method and application of silicon-boron-nitrogen fiber reinforced boron nitride ceramic matrix composite material
CN114702328A (en) SiC nanowire network reinforced layered porous SiC ceramic and preparation method thereof
CN114920574A (en) Method for preparing large-size carbon-carbon crucible by three-dimensional weaving of carbon fibers
CN112060620A (en) Carbon-carbon heat-preserving cylinder forming process
KR20020066547A (en) Method for manufacturing carbon/silicon-carbide composite
CN115160007B (en) Carbon-carbon composite structure and preparation method thereof
CN105565838A (en) Method for manufacturing ceramic-based composite burners for field of coal chemical industry
CN115141029B (en) Preparation method of carbon/carbon crucible support rod
RU2568495C1 (en) Method of producing carbon-carbon composite material based on carbon fibre filler and carbon matrix
CN117024164A (en) Ceramic modified carbon-carbon composite nose cone and preparation method thereof
KR20100116780A (en) Method for forming ceramic fiber preform of ceramic composite
CN115259882A (en) Production process of composite fiber filament winding carbon-carbon composite material
CN115572174A (en) Preparation method of carbon-carbon composite material, carbon-carbon composite material and application thereof
CN110550963B (en) Preparation method of thin-wall C/SiC extension section
CN114890805A (en) Preparation process of carbon-carbon crucible in continuous graphitizing furnace

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant